CN108539237B - Nafion composite membrane modified by silver/platinum nano catalyst and preparation method thereof - Google Patents
Nafion composite membrane modified by silver/platinum nano catalyst and preparation method thereof Download PDFInfo
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- CN108539237B CN108539237B CN201810421902.0A CN201810421902A CN108539237B CN 108539237 B CN108539237 B CN 108539237B CN 201810421902 A CN201810421902 A CN 201810421902A CN 108539237 B CN108539237 B CN 108539237B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1041—Polymer electrolyte composites, mixtures or blends
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
A Nafion composite membrane modified by silver/platinum nano-catalyst and a preparation method thereof relate to a Nafion composite membrane. The Nafion composite membrane is provided with a Nafion membrane and a silver/platinum bimetallic nano catalyst, the catalyst is loaded on the Nafion membrane, and the catalyst directly grows on the Nafion membrane. Soaking Nafion membrane in sodium salt solution to obtain Nafion-Na with Na ions on surface+Molding a film; mixing Nafion-Na+Soaking the molded film in silver salt solution to obtain Nafion-Ag with Ag ions on the surface+Molding a film; mixing Nafion-Ag+Immersing the shaped membrane into a mixed solution of a surfactant and a reducing agent, heating the mixed solution, adding a reaction initiator for reaction, and obtaining a Nafion-Ag shaped membrane with Ag nano particles growing on the surface; and soaking the Nafion-Ag type membrane in a platinum salt solution to obtain the Nafion composite membrane modified by the silver/platinum nano catalyst.
Description
Technical Field
The invention relates to a Nafion composite membrane, in particular to a Nafion composite membrane modified by a silver/platinum nano catalyst and a preparation method thereof.
Background
A fuel cell is an energy conversion device that directly converts chemical energy of a fuel and an oxidant into electrical energy. The novel energy automobile power generation system has the advantages of high energy conversion rate, few pollutants during operation, low noise and the like, and is considered to be one of the development directions of new energy automobile power. However, a Membrane Electrode Assembly (MEA), which is one of the key components of the fuel cell, is expensive to manufacture, and has the disadvantages of low output power, poor stability, and the like, which greatly hinders the large-scale application of the fuel cell.
The cost of MEA is high because the precious metal platinum catalyst is used to catalyze the electrode reaction of fuel cell, but the current platinum catalyst has low catalytic activity for the oxygen reduction reaction of the cathode of fuel cell, and a large amount of platinum catalyst needs to be used in MEA to ensure the output power of MEA to meet the requirement of practical application, which greatly increases the cost of MEA.
There are two types of approaches to solve this problem, one is to improve the platinum catalyst and increase the intrinsic catalytic activity of platinum metal while reducing the amount of platinum metal, for example, M.Markovic published in Science (Science,2007,315:493 497) reports that the electrocatalytic activity is much higher than that of Pt single crystal material3A Ni alloy material; journal of Power Sources paper (Journal of Power Sources,2017,365:17-25) published by Tao et al reports Ag/Pt bimetallic catalysts with higher oxygen reduction catalytic activity than commercial Pt/C catalysts. The other is to improve the preparation process of the MEA, so that the catalytic layer structure in the MEA is more suitable for catalyzing the reaction of gas. Such as vacuum sputtering, chemical deposition, electrochemical deposition, and the like, in which a metal catalyst is directly deposited on a Nafion membrane. Srinivasan et al have reported that the loading of MEA prepared by spraying Pt particles on a proton exchange membrane is much lower than that of MEA prepared by the conventional method, and the microstructure of the catalytic layer of the MEA is improved and has a certain output power (electrochim. acta,1997,42: 1587-. Therefore, the method has certain functions and potential in practical application.
Disclosure of Invention
The invention aims to provide a Nafion composite membrane modified by a silver/platinum nano catalyst and a preparation method thereof aiming at the prior technical problems.
The Nafion composite membrane modified by the silver/platinum nano-catalyst is provided with a Nafion membrane and a silver/platinum bimetallic nano-catalyst, wherein the silver/platinum bimetallic nano-catalyst is loaded on the Nafion membrane, the size of the silver/platinum bimetallic nano-catalyst can be 4-300 nm, the Pt loading capacity can be regulated, and the thickness of the Nafion membrane can be 25-200 mu m. The Nafion composite membrane modified by the silver/platinum nano-catalyst takes a silver/platinum bimetallic material as a catalyst, so that the dosage of platinum in the catalyst is reduced, and the cost is lower than that of a material using pure platinum; in addition, the Nafion composite membrane modified by the silver/platinum nano-catalyst can be directly hot-pressed with carbon paper to form an MEA, so that the preparation difficulty of the MEA is greatly reduced, and the manufacturing cost of the MEA can be reduced. The preparation method is simple to operate and high in repeatability; the prepared composite membrane has low cost, higher electrocatalytic activity and catalytic stability, and can be applied to the energy field of fuel cells and the like.
The preparation method of the Nafion composite membrane modified by the silver/platinum nano catalyst comprises the following steps:
1) soaking Nafion membrane in sodium salt solution to obtain Nafion-Na with Na ions on surface+Molding a film;
2) mixing Nafion-Na+Soaking the molded film in silver salt solution to obtain Nafion-Ag with Ag ions on the surface+Molding a film;
3) mixing Nafion-Ag+Immersing the shaped membrane into a mixed solution of a surfactant and a reducing agent, heating the mixed solution, and adding a reaction initiator for reaction to obtain a Nafion-Ag shaped membrane with Ag nano particles growing on the surface;
4) and soaking the Nafion-Ag type membrane in a platinum salt solution to obtain a Nafion composite membrane modified by the silver/platinum nano catalyst, namely the Nafion-Ag/Pt type membrane with the Ag/Pt bimetallic nano catalyst growing on the surface.
In the step 1), the thickness of the Nafion film can be 25-200 μm, and the sodium salt used in the sodium salt solution can be one selected from sodium sulfate, sodium nitrate, sodium carbonate, sodium chloride and the like; the mass concentration of the sodium salt can be 0.000-1.000M; the temperature of the sodium salt solution can be 0-100 ℃; the soaking time can be 0-48 h.
In step 2), the silver salt used in the silver salt solution can be selected from one of silver carbonate, silver nitrate, silver sulfate and the like; the mass concentration of the silver salt can be 0.001-1.000M; the temperature of the silver salt solution can be 0-100 ℃; the soaking time can be 1-48 h.
In step 3), the surfactant in the mixed solution can be one selected from oleic acid, polyvinylpyrrolidone, glucose, polyethylene glycol and the like; the mass concentration of the surfactant in the mixed solution can be 0.000-5.000M; the reducing agent in the mixed solution can be one of ascorbic acid, sodium citrate, sodium sulfite, sodium hypophosphite and the like; the mass concentration of the reducing agent in the mixed solution can be 0.001-1.000M; the mixed solution needs to be heated to 15-100 ℃; the reaction initiator can be selected from one of sodium hypophosphite, lithium aluminum hydride, sodium borohydride and the like; the addition amount of the reaction initiator is that the mass concentration of the added reaction initiator in the mixed solution is 0.001-0.100M; the reaction time can be 1-48 h.
In step 4), the platinum salt used in the platinum salt solution may be selected from one of chloroplatinic acid, potassium hexachloroplatinate, potassium tetrachloroplatinate, platinum nitrate, etc.; the mass concentration of the platinum salt can be 0.001-1.000M; the temperature of the platinum salt solution can be 0-100 ℃; the soaking time can be 1-48 h.
The invention is composed of a Nafion film and a silver/platinum bimetallic nano-catalyst which uniformly grows on the Nafion film, and the combination of the metal catalyst and the Nafion film is very firm. The size of the silver/platinum nano catalyst is 4-300 nm, the Pt loading capacity can be regulated, and the thickness of the Nafion film is 25-200 mu m. The preparation method is simple to operate and high in repeatability; the prepared composite membrane has low cost, higher electrocatalytic activity and catalytic stability, and can be applied to the energy field of fuel cells and the like.
Drawings
Figure 1 is a photograph of a low metal loading Nafion composite membrane of example 1.
FIG. 2 is a scanning electron micrograph of a Nafion composite film with low metal loading of example 1.
FIG. 3 is a scanning electron micrograph of the metal loaded Nafion composite film of example 2.
FIG. 4 is a scanning electron micrograph of the Nafion composite film with high metal loading of example 3.
FIG. 5 is a scanning electron micrograph and elemental distribution scan of a cross section of a Nafion composite film with low metal loading of example 4.
FIG. 6 is a scanning electron micrograph and elemental distribution scan of a cross section of a metal loaded Nafion composite membrane of example 5.
Detailed Description
The preparation method and the preparation method of the Nafion composite membrane modified by the silver/platinum nano catalyst are further described by the embodiment in combination with the attached drawings.
Example 1
Soaking a Nafion membrane with the thickness of 25 mu M in a 0.000M sodium carbonate solution at 0 ℃ for 0h, taking out and soaking in a 0.001M silver sulfate solution at 0 ℃ for 1h, then soaking in a mixed solution of 0.000M oleic acid and 0.001M sodium hypophosphite, heating the mixed solution to 15 ℃, adding 0.001M lithium aluminum hydride, reacting for 1h to obtain a Nafion-Ag type membrane with Ag nano particles growing on the surface, and soaking in a 0.001M potassium hexachloroplatinate solution for 1h to obtain the Nafion composite membrane modified by the silver/platinum nano catalyst with low platinum loading. The picture of the low metal loading Nafion composite membrane is shown in figure 1, and the scanning electron microscope picture of the low metal loading Nafion composite membrane is shown in figure 2.
Example 2
Soaking a Nafion membrane with the thickness of 50 mu M in a 0.001M sodium sulfate solution at 25 ℃ for 5 hours, taking out the Nafion membrane and soaking the Nafion membrane in a 0.002M silver carbonate solution at 25 ℃ for 10 hours, soaking the Nafion membrane in a mixed solution of 0.001M glucose and 0.002M ascorbic acid, heating the mixed solution to 25 ℃, adding 0.002M sodium hypophosphite, reacting for 5 hours to obtain a Nafion-Ag type membrane with Ag nano particles growing on the surface, and soaking the Nafion-Ag type membrane in a 0.002M chloroplatinic acid solution for 10 hours to obtain the Nafion composite membrane modified by the silver/platinum nano catalyst with medium platinum loading. See figure 3 for a scanning electron micrograph of a metal loaded Nafion composite membrane.
Example 3
Soaking a 75-micrometer Nafion membrane in a 1.000-M sodium nitrate solution at 100 ℃ for 48 hours, taking out the Nafion membrane, soaking the Nafion membrane in a 1.000-M silver nitrate solution at 100 ℃ for 48 hours, soaking the Nafion membrane in a mixed solution of 5.000-M polyethylene glycol and 1.000-M sodium sulfite, heating the mixed solution to 100 ℃, adding 0.100-M sodium borohydride, reacting for 48 hours to obtain a Nafion-Ag type membrane with Ag nanoparticles growing on the surface, and soaking the Nafion-Ag type membrane in a 1.000-M platinum nitrate solution for 48 hours to obtain the Nafion composite membrane modified by the silver/platinum nano catalyst with high platinum loading capacity. A scanning electron micrograph of a high metal loading Nafion composite membrane is shown in figure 4.
Example 4
Soaking a Nafion membrane with the thickness of 200 mu M in 0.010M sodium chloride solution at 5 ℃ for 30 hours, taking out the Nafion membrane and soaking the Nafion membrane in 0.500M silver nitrate solution at 5 ℃ for 40 hours, soaking the Nafion membrane in a mixed solution of 3.000M polyvinylpyrrolidone and 0.800M sodium citrate, heating the mixed solution to 80 ℃, adding 0.080M sodium hypophosphite into the mixed solution, reacting for 35 hours to obtain a Nafion-Ag type membrane with Ag nano particles growing on the surface, and soaking the Nafion-Ag type membrane in 0.700M potassium tetrachloroplatinate solution for 18 hours to obtain the Nafion composite membrane modified by the silver/platinum nano catalyst with low platinum loading capacity. The effect is the same as in example 1. The scanning electron micrograph and the element distribution scan of the cross section of the Nafion composite membrane with low metal loading are shown in fig. 5.
Example 5
Soaking a Nafion membrane with the thickness of 100 mu M in 0.100M sodium nitrate solution at 85 ℃ for 10 hours, taking out and soaking in 0.900M silver sulfate solution at 65 ℃ for 8 hours, soaking in a mixed solution of 2.500M oleic acid and 0.400M ascorbic acid, heating the mixed solution to 30 ℃, adding 0.030M sodium borohydride, reacting for 45 hours to obtain a Nafion-Ag type membrane with Ag nanoparticles growing on the surface, and soaking in 0.900M potassium tetrachloroplatinate solution for 7 hours to obtain the Nafion composite membrane modified by the silver/platinum nano catalyst with the medium platinum loading. The effect is the same as in example 2. The scanning electron micrograph and the elemental distribution scan of the cross section of the metal loaded Nafion composite membrane are shown in fig. 6.
Claims (8)
1. The Nafion composite membrane modified by the silver/platinum nano catalyst is characterized by being provided with a Nafion membrane and a silver/platinum bimetallic nano catalyst, wherein the silver/platinum bimetallic nano catalyst is loaded on the Nafion membrane, the Pt loading capacity is adjustable, the Nafion composite membrane modified by the silver/platinum nano catalyst takes a silver/platinum bimetallic material as a catalyst, and the silver/platinum bimetallic nano catalyst directly grows on the Nafion membrane; the size of the silver/platinum bimetallic nano-catalyst is 4-300 nm;
the preparation method of the Nafion composite membrane modified by the silver/platinum nano catalyst is characterized by comprising the following steps:
1) soaking Nafion membrane in sodium salt solution to obtain Nafion-Na with Na ions on surface+Molding a film;
2) mixing Nafion-Na+Soaking the formed film in silver salt solutionIn the solution, Nafion-Ag with Ag ions on the surface is obtained+Molding a film;
3) mixing Nafion-Ag+Immersing the shaped membrane into a mixed solution of a surfactant and a reducing agent, heating the mixed solution, and adding a reaction initiator for reaction to obtain a Nafion-Ag shaped membrane with Ag nano particles growing on the surface;
4) and soaking the Nafion-Ag type membrane in a platinum salt solution to obtain a Nafion composite membrane modified by the silver/platinum nano catalyst, namely the Nafion-Ag/Pt type membrane with the Ag/Pt bimetallic nano catalyst growing on the surface.
2. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein the Nafion membrane has a thickness of 25 to 200 μm.
3. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein in the step 1), the sodium salt used in the sodium salt solution is selected from one of sodium sulfate, sodium nitrate, sodium carbonate and sodium chloride; the mass concentration of the sodium salt is 0.000-1.000M; the temperature of the sodium salt solution is 0-100 ℃; the soaking time is 0-48 h.
4. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein in the step 2), the silver salt used in the silver salt solution is selected from one of silver carbonate, silver nitrate and silver sulfate; the mass concentration of the silver salt is 0.001-1.000M; the temperature of the silver salt solution is 0-100 ℃; the soaking time is 1-48 h.
5. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein in the step 3), the surfactant in the mixed solution is selected from one of oleic acid, polyvinylpyrrolidone, glucose and polyethylene glycol; the mass concentration of the surfactant in the mixed solution is 0.000-5.000M.
6. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein in the step 3), the reducing agent in the mixed solution is selected from one of ascorbic acid, sodium citrate, sodium sulfite and sodium hypophosphite; the mass concentration of the reducing agent in the mixed solution is 0.001-1.000M; the mixed solution needs to be heated to 15-100 ℃.
7. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein in the step 3), the reaction initiator is selected from one of sodium hypophosphite, lithium aluminum hydride and sodium borohydride; the addition amount of the reaction initiator is that the mass concentration of the added reaction initiator in the mixed solution is 0.001-0.100M; the reaction time is 1-48 h.
8. The silver/platinum nanocatalyst modified Nafion composite membrane as claimed in claim 1, wherein in the step 4), the platinum salt used in the platinum salt solution is selected from one of chloroplatinic acid, potassium hexachloroplatinate, potassium tetrachloroplatinate and platinum nitrate; the mass concentration of the platinum salt is 0.001-1.000M; the temperature of the platinum salt solution is 0-100 ℃; the soaking time is 1-48 h.
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| CN109546159A (en) * | 2018-11-22 | 2019-03-29 | 龙岩学院 | A kind of very thin fuel cell catalyst layer and preparation method thereof |
| CN113285107B (en) * | 2021-04-27 | 2022-03-29 | 大连理工大学 | Integrated membrane electrode with ultralow precious metal loading capacity and preparation method and application thereof |
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